CN113063769A - Magnetic induction assembled Fe3O4Preparation method of @ PPy @ Ag array type SERS substrate - Google Patents

Magnetic induction assembled Fe3O4Preparation method of @ PPy @ Ag array type SERS substrate Download PDF

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CN113063769A
CN113063769A CN202110317979.5A CN202110317979A CN113063769A CN 113063769 A CN113063769 A CN 113063769A CN 202110317979 A CN202110317979 A CN 202110317979A CN 113063769 A CN113063769 A CN 113063769A
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ppy
sers substrate
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assembled
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程琳
季善鹏
刘爱萍
许为中
王晶晶
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Zhejiang University of Technology ZJUT
Zhejiang Sci Tech University ZSTU
Zhejiang University of Science and Technology ZUST
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
    • G01N21/65—Raman scattering
    • G01N21/658—Raman scattering enhancement Raman, e.g. surface plasmons
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05—Metallic powder characterised by the size or surface area of the particles
    • B22F1/054—Nanosized particles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/07—Metallic powder characterised by particles having a nanoscale microstructure
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/17—Metallic particles coated with metal
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures

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Abstract

The invention provides a magnetic induction assembled Fe3O4Preparation method of @ PPy @ Ag array type SERS substrate to prepare monodisperse Fe3O4The @ PPy @ Ag nano composite particles are SERS substrate construction units, and Fe is prepared by the co-induction assembly of an external reinforcing magnet and a nano imprinting hole template3O4The method is simple to operate, and large-scale construction of the array type SERS substrate with high active hot spot density can be realized.

Description

Magnetic induction assembled Fe3O4Preparation method of @ PPy @ Ag array type SERS substrate
Technical Field
The invention relates to the field of nano material preparation, in particular to magnetic induction assembled Fe3O4A preparation method of the @ PPy @ Ag array type SERS substrate.
Background
The surface enhanced Raman scattering technology can obtain the component and structural information of substance molecules, can provide nondestructive, qualitative and quantitative detection and analysis, and has the characteristics of high detection speed and simple operation, thereby becoming an important means for environmental monitoring. The key of the SERS technology lies in the construction of a high-activity and high-stability SERS substrate.
The array type SERS substrate is generally prepared or grown on a substrate to be array arrangement, the preparation method mainly comprises a template method, electron beam etching, electrodeposition and the like, and the structure of the substrate is characterized in that active 'hot spots' are periodically arranged and are uniformly dispersed, so that the signal obtained on the whole film substrate has good repeatability and high stability, but due to the limitation of the preparation method, the particle gap is difficult to control in the nanometer level, and the density of the active 'hot spots' is not high. Therefore, a novel preparation method is urgently needed to be developed to construct the array type SERS substrate with high-activity hot spot density.
Disclosure of Invention
In order to solve the technical problems, the invention provides a magnetic induction assembled Fe3O4Preparation method of @ PPy @ Ag array type SERS substrate, and Fe is used in method3O4Is a core material, the surface of the core material is modified with polypyrrole and then is coated with a nano silver shell layer, and Fe with high active hot spot density is prepared3O4The @ PPy @ Ag nano composite particle is realized by using Fe through an external magnetic field and a nano imprinting hole template3O4And preparing the array type SERS substrate with the @ PPy @ Ag nano composite particles as substrate construction units.
In order to achieve the technical purpose, the technical scheme of the invention is as follows:
magnetic induction assembled Fe3O4The preparation method of the @ PPy @ Ag array type SERS substrate comprises the following steps:
step 1; preparation of monodisperse Fe by solvothermal method3O4Nanoparticles of Fe3O4Sequentially coating polypyrrole and Ag nanoparticles on the outer surface of the nanoparticles to obtain single componentsBulk Fe3O4@ PPy @ Ag nanocomposite particles;
step 2; subjecting said monodisperse Fe3O4The @ PPy @ Ag nano composite particles are dispersed in an aqueous solution for ultrasonic dispersion and are uniformly stirred to obtain Fe3O4@ PPy @ Ag nano composite particle solution, adding Fe3O4Dripping the @ PPy @ Ag nano composite particle solution onto a nano imprinting hole template, wherein a strong magnet is arranged at the bottom of the nano imprinting hole template;
step 3; slowly moving the strong magnet to make the Fe3O4Assembling the @ PPy @ Ag nano composite particles into the nano imprinting hole template to obtain Fe3O4An array arrangement SERS substrate assembled by @ PPy @ Ag composite particles;
step 4; subjecting said Fe to3O4The array arrangement SERS substrate assembled by the @ PPy @ Ag composite particles is used for Raman testing of organic pollutant molecules.
Preferably, the Fe3O4The preparation steps of the nano-particles are as follows: respectively dissolving ferric trichloride hexahydrate and sodium acetate into equivalent ethylene glycol according to the mass ratio of 1:10, then uniformly mixing and stirring the two solutions, adding 10-30 wt% of polyacrylic acid solution, continuously stirring for 6-12h, then transferring into a reaction kettle, and keeping the reaction for 4-12 h at the temperature of 180-210 ℃ to obtain a black product Fe3O4Nanoparticles, wherein the Fe3O4The size of the nano particles is 100-250 nm.
Preferably, the Fe is3O4Adding ethanol and water into the nanoparticles in a ratio of 1:1, performing ultrasonic dispersion, adding 10-50 mu L of pyrrole, uniformly stirring, finally adding 6mol/L hydrochloric acid solution, performing water bath ultrasonic reaction, performing alternate centrifugal cleaning by using deionized water and ethanol, and performing surface modification by using PPy to obtain the Fe3O4@ PPy nanocomposite particles.
Further, said Fe3O4Preparing the @ PPy composite particles into 5-20 mg/mL aqueous solution, adding the aqueous solution into the silver-ammonia solution prepared from ammonia water and silver nitrate, and placing the solution into a shaking table to shake for 8-16 hoursMagnetically separating to obtain said monodisperse Fe3O4@ PPy @ Ag nanocomposite particles.
Preferably, the monodisperse Fe3O4The @ PPy @ Ag nano composite particles are dispersed into an aqueous solution, the preparation concentration is 1-20mg/L, and the nano composite particles are dropwise added onto a nano imprinting hole template.
Preferably, the nanoimprint pore template has adjustable experimental parameters, the experimental parameters including: period parameter, aperture, height and mode of arrangement, wherein, the mode of arrangement includes: rectangular, hexagonal, triangular.
Compared with the prior art, the invention has the following beneficial effects:
1. the invention provides a process for preparing Fe3O4The @ PPy @ Ag composite particles are SERS substrate construction units, and Fe is prepared by combining external magnets with nanoimprint pore templates3O4The method for @ PPy @ Ag array type SERS substrate is simple to operate, and large-scale construction of the array type SERS substrate with high active hot spot density can be achieved.
2. Fe prepared by the invention3O4The @ PPy @ Ag array type SERS substrate can regulate and control Fe3O4The shape structure of @ PPy @ Ag enhances the sensitivity of SERS substrate signals, and the distance between particles can be adjusted by adjusting the structural period parameters of the nanoimprint hole template, so that the better SERS performance is achieved.
3. The invention provides magnetic induction assembled Fe3O4The preparation method of the @ PPy @ Ag array type SERS substrate can be suitable for constructing other high-performance SERS substrates based on magnetic-based noble metal nanocomposite materials.
Drawings
FIG. 1 shows Fe obtained in example 1 of the present invention3O4Scanning electron microscopy images of @ PPy @ Ag.
FIG. 2 is a scanning electron microscope image of the nanoimprinted pore template obtained in example 1 of the present invention.
FIG. 3 shows the magnetically induced assembly of Fe obtained in example 1 of the present invention3O4Scanning electron microscopy images of an array-type SERS substrate of @ PPy @ Ag.
FIG. 4 shows the magnetically induced assembly of Fe obtained in example 2 of the present invention3O4Scanning electron microscopy images of an array-type SERS substrate of @ PPy @ Ag.
Detailed Description
In order to make the technical problems, technical solutions and advantages of the present invention more apparent, the following detailed description is given with reference to the accompanying drawings and specific embodiments. In the following description, characteristic details such as specific configurations and components are provided only to help the embodiments of the present invention be fully understood. Thus, it will be apparent to those skilled in the art that various changes and modifications may be made to the embodiments described herein without departing from the scope and spirit of the invention. In addition, descriptions of well-known functions and constructions are omitted for clarity and conciseness.
It should be appreciated that reference throughout this specification to "one embodiment" or "an embodiment" means that a particular feature, structure or characteristic described in connection with the embodiment is included in at least one embodiment of the present invention. Thus, the appearances of the phrases "in one embodiment" or "in an embodiment" in various places throughout this specification are not necessarily all referring to the same embodiment. Furthermore, the particular features, structures, or characteristics may be combined in any suitable manner in one or more embodiments.
In various embodiments of the present invention, it should be understood that the sequence numbers of the following processes do not mean the execution sequence, and the execution sequence of each process should be determined by its function and inherent logic, and should not constitute any limitation to the implementation process of the embodiments of the present invention.
It should be understood that the term "and/or" herein is merely one type of association relationship that describes an associated object, meaning that three relationships may exist, e.g., a and/or B may mean: a exists alone, A and B exist simultaneously, and B exists alone. In addition, the character "/" herein generally indicates that the former and latter related objects are in an "or" relationship.
In the embodiments provided herein, it should be understood that "B corresponding to a" means that B is associated with a from which B can be determined. It should also be understood that determining B from a does not mean determining B from a alone, but may be determined from a and/or other information.
With reference to the attached drawings 1-4, the invention provides a magnetic induction assembled Fe3O4The preparation method of the @ PPy @ Ag array type SERS substrate comprises the following steps:
step 1; preparation of monodisperse Fe by solvothermal method3O4Nanoparticles of in Fe3O4Sequentially coating polypyrrole and Ag nanoparticles on the outer surface of the nanoparticles to prepare monodisperse Fe3O4@ PPy @ Ag nanocomposite particles.
Further elaboration, Fe3O4The preparation steps of the nano-particles are as follows: respectively dissolving ferric trichloride hexahydrate and sodium acetate into equivalent ethylene glycol according to the mass ratio of 1:10, then uniformly mixing and stirring the two solutions, adding 10-30 wt% of polyacrylic acid solution, continuously stirring for 6-12h, then transferring into a reaction kettle, and keeping the reaction for 4-12 h at the temperature of 180-210 ℃ to obtain a black product Fe3O4Nanoparticles of which Fe3O4The size of the nano particles is 100-250 nm.
Further, Fe3O4Adding ethanol and water into the nanoparticles in a ratio of 1:1, performing ultrasonic dispersion, adding 10-50 mu L of pyrrole, uniformly stirring, finally adding 6mol/L hydrochloric acid solution, performing water bath ultrasonic reaction, performing alternate centrifugal cleaning by using deionized water and ethanol, and performing surface modification by using PPy to obtain Fe3O4@ PPy nanocomposite particles.
Further, Fe3O4Preparing the @ PPy composite particles into 5-20 mg/mL aqueous solution, adding the aqueous solution into a silver-ammonia solution prepared from ammonia water and silver nitrate, placing the solution into a shaking table, shaking for 8-16 hours, and carrying out magnetic separation to obtain monodisperse Fe3O4@ PPy @ Ag nanocomposite particles.
Step 2; monodisperse Fe3O4The @ PPy @ Ag nano composite particles are dispersed in an aqueous solution for ultrasonic dispersion and are uniformly stirred to obtain Fe3O4@ PPy @ Ag nano composite particle solution, mixing Fe3O4Dripping @ PPy @ Ag nano composite particle solution onto a nano imprinting hole templateWherein, the bottom of the nanometer impressing hole template is provided with a strong magnet.
Further illustrating that monodisperse Fe3O4The @ PPy @ Ag nano composite particles are dispersed into an aqueous solution, the preparation concentration is 1-20mg/L, and the nano composite particles are dropwise added onto a nano imprinting hole template.
Further illustrating that the experimental parameters of the nanoimprint aperture template are adjustable, including: period parameter, aperture, height and mode of arrangement, wherein, the mode of arrangement includes: rectangular, hexagonal, triangular.
Step 3; slowly moving the strong magnet to make the Fe3O4Assembling the @ PPy @ Ag nano composite particles into a nano imprinting hole template to obtain Fe3O4Array arrangement SERS substrate assembled by @ PPy @ Ag composite particles.
Further, the magnet placed at the bottom is slowly moved so that Fe3O4The @ PPy @ Ag composite particles realize array arrangement.
Step 4; mixing Fe3O4The array arrangement SERS substrate assembled by the @ PPy @ Ag composite particles is used for Raman testing of organic pollutant molecules.
In the case of the example 1, the following examples are given,
respectively dissolving 1.8mg of ferric trichloride hexahydrate and 18mg of sodium acetate into 40ml of ethylene glycol, then uniformly mixing and stirring the two solutions, adding 10 wt% of polyacrylic acid solution, continuously stirring for 6 hours, then transferring to a polytetrafluoroethylene reaction kettle, and keeping the reaction for 8 hours at 202 ℃ to obtain ferroferric oxide nanoparticles with the size of 150 nm; taking prepared Fe3O4Adding 10mg of nano particles into a mixed solution of 20ml of ethanol and 20ml of water, fully and ultrasonically dispersing for 30min, then adding 10 mu L of pyrrole, uniformly stirring, then adding 3ml of hydrochloric acid with the concentration of 6mol/L, carrying out ultrasonic reaction for 90min at 25 ℃ in a water bath, and then alternately centrifuging and cleaning for 3 times by using deionized water and ethanol to obtain the Fe-B nano particle3O4@ PPy composite particles. Fe prepared as above3O4Preparing the @ PPy composite particles into 5mg/mL aqueous solution, adding 10mL of aqueous solution into 1mL of silver-ammonia solution prepared from ammonia water and silver nitrate, placing the solution into a shaking table, shaking for 12 hours, and carrying out magnetic separation to obtain Fe3O4The scanning electron microscope picture of the @ PPy @ Ag composite particle is shown in FIG. 1. Fe to be produced3O4The @ PPy @ Ag composite particles are dispersed into an aqueous solution, the configuration concentration is 3mg/L, the particles are dropwise added to a nano-imprinting hole template with a magnet placed at the bottom, the nano-imprinting hole template is arranged in a hexagon mode as shown in a Scanning Electron Microscope (SEM) of figure 2, the period parameter is 200nm, the aperture is 100nm, the height is 100nm, the magnet placed at the bottom is slowly moved, and the dropwise added Fe is enabled to be3O4The @ PPy @ Ag composite particles realize array arrangement, and the assembled Fe is obtained3O4The @ PPy @ Ag array type SERS substrate is shown in figure 3 by a scanning electron microscope picture.
In the case of the example 2, the following examples are given,
respectively dissolving 1.8mg of ferric trichloride hexahydrate and 18mg of sodium acetate into 40ml of ethylene glycol, mixing and stirring the two solutions uniformly, adding 10 wt% of polyacrylic acid solution, continuously stirring for 6 hours, transferring to a polytetrafluoroethylene reaction kettle, and keeping the reaction for 8 hours at 202 ℃ to obtain 150 nm-sized Fe3O4A nanoparticle; taking prepared Fe3O4Adding 10mg of nano particles into a mixed solution of 20ml of ethanol and 20ml of water, fully and ultrasonically dispersing for 30min, then adding 50 mu L of pyrrole, uniformly stirring, then adding 3ml of hydrochloric acid with the concentration of 6mol/L, carrying out ultrasonic reaction for 120min at 25 ℃ in a water bath, and then alternately centrifuging and cleaning for 3 times by using deionized water and ethanol to obtain Fe3O4@ PPy composite particles. Fe prepared as above3O4Preparing the @ PPy composite particles into 5mg/mL aqueous solution, taking out 10mL, adding the aqueous solution into 10mL silver ammonia solution prepared from ammonia water and silver nitrate, placing the solution into a shaking table, shaking for 12 hours, and carrying out magnetic separation to obtain Fe3O4@ PPy @ Ag composite particles. Mixing Fe prepared in the step one3O4In the aqueous solution is dispersed to @ PPy @ Ag composite particle, the configuration concentration is 10mg/L, drip dropwise on the nanometer impression hole template of magnet is placed to the bottom, nanometer impression hole template arranges for the hexagon, and the cycle parameter is 200nm, and the aperture is 100nm, highly is 100nm, and the magnet of slowly moving bottom placing for dropwise Fe3O4The @ PPy @ Ag composite particles realize array arrangement, and the assembled Fe is obtained3O4The @ PPy @ Ag array type SERS substrate is shown in figure 4 by a scanning electron microscope picture.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the invention has been described in detail with reference to the foregoing illustrative embodiments, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the spirit and scope of the technical solutions of the embodiments of the present invention.

Claims (6)

1. Magnetic induction assembled Fe3O4The preparation method of the @ PPy @ Ag array type SERS substrate is characterized by comprising the following steps:
step 1; preparation of monodisperse Fe by solvothermal method3O4Nanoparticles of Fe3O4Sequentially coating polypyrrole and Ag nanoparticles on the outer surface of the nanoparticles to prepare monodisperse Fe3O4@ PPy @ Ag nanocomposite particles;
step 2; subjecting said monodisperse Fe3O4The @ PPy @ Ag nano composite particles are dispersed in an aqueous solution for ultrasonic dispersion and are uniformly stirred to obtain Fe3O4@ PPy @ Ag nano composite particle solution, adding Fe3O4Dripping the @ PPy @ Ag nano composite particle solution onto a nano imprinting hole template, wherein a strong magnet is arranged at the bottom of the nano imprinting hole template;
step 3; slowly moving the strong magnet to make the Fe3O4Assembling the @ PPy @ Ag nano composite particles into the nano imprinting hole template to obtain Fe3O4An array arrangement SERS substrate assembled by @ PPy @ Ag composite particles;
step 4; subjecting said Fe to3O4The array arrangement SERS substrate assembled by the @ PPy @ Ag composite particles is used for Raman testing of organic pollutant molecules.
2. According toA magnetically induced assembled Fe of claim 13O4The preparation method of the @ PPy @ Ag array type SERS substrate is characterized in that Fe3O4The preparation steps of the nano-particles are as follows: respectively dissolving ferric trichloride hexahydrate and sodium acetate into equivalent ethylene glycol according to the mass ratio of 1:10, then uniformly mixing and stirring the two solutions, adding 10-30 wt% of polyacrylic acid solution, continuously stirring for 6-12h, then transferring into a reaction kettle, and keeping the reaction for 4-12 h at the temperature of 180-210 ℃ to obtain a black product Fe3O4Nanoparticles, wherein the Fe3O4The size of the nano particles is 100-250 nm.
3. A magnetically induced assembled Fe according to claim 13O4The preparation method of the @ PPy @ Ag array type SERS substrate is characterized in that Fe3O4Adding ethanol and water into the nanoparticles in a ratio of 1:1, performing ultrasonic dispersion, adding 10-50 mu L of pyrrole, uniformly stirring, finally adding 6mol/L hydrochloric acid solution, performing water bath ultrasonic reaction, performing alternate centrifugal cleaning by using deionized water and ethanol, and performing surface modification by using PPy to obtain the Fe3O4@ PPy nanocomposite particles.
4. A magnetically induced assembled Fe according to claim 33O4The preparation method of the @ PPy @ Ag array type SERS substrate is characterized in that Fe3O4Preparing the @ PPy composite particles into 5-20 mg/mL aqueous solution, adding the aqueous solution into a silver-ammonia solution prepared from ammonia water and silver nitrate, placing the solution into a shaking table, shaking for 8-16 hours, and carrying out magnetic separation to obtain the monodisperse Fe3O4@ PPy @ Ag nanocomposite particles.
5. A magnetically induced assembled Fe according to claim 13O4The preparation method of the @ PPy @ Ag array type SERS substrate is characterized in that the monodisperse Fe3O4The @ PPy @ Ag nano composite particles are dispersed into an aqueous solution, the preparation concentration is 1-20mg/L, and the nano composite particles are dropwise added onto a nano imprinting hole template.
6. A magnetically induced assembled Fe according to claim 13O4The preparation method of the @ PPy @ Ag array type SERS substrate is characterized in that the experimental parameters of the nanoimprint hole template are adjustable, and the experimental parameters comprise: period parameter, aperture, height and mode of arrangement, wherein, the mode of arrangement includes: rectangular, hexagonal, triangular.
CN202110317979.5A 2021-03-25 2021-03-25 Magnetic induction assembled Fe3O4Preparation method of @ PPy @ Ag array type SERS substrate Pending CN113063769A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113713782A (en) * 2021-08-16 2021-11-30 中化学朗正环保科技有限公司 Silver @ polypyrrole composite material for wastewater adsorption and preparation method and application thereof
CN114767854A (en) * 2022-04-22 2022-07-22 浙江理工大学 Preparation method of nano composite microsphere for enhancing magnetocaloric and photothermal properties

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113713782A (en) * 2021-08-16 2021-11-30 中化学朗正环保科技有限公司 Silver @ polypyrrole composite material for wastewater adsorption and preparation method and application thereof
CN113713782B (en) * 2021-08-16 2024-02-06 中化学朗正环保科技有限公司 Silver@polypyrrole composite material for wastewater adsorption and preparation method and application thereof
CN114767854A (en) * 2022-04-22 2022-07-22 浙江理工大学 Preparation method of nano composite microsphere for enhancing magnetocaloric and photothermal properties

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